Electrolytic process of producing nitrogen compounds.



O. E. AOKER.

ELECTROLYTIC PROCESS OF PRODUCING NITROGEN COMPOUNDS.

APPLIUATION FILED 0018,1906.

914,214,, Patented Mar. 2, 1909.

2 SHEETS-SHEET 1.

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C. E. ACKER.

ELECTROLYTIC PROCESS OF PRODUCING NITROGEN COMPOUNDS.

APPLICATION FILED OCT.8,1906.

914,214., Patented Mar. 2, 1909.

2 SHEETS-SHEET 2.

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CHARLES E. AOKER, OF NIAGARA FALLS, NEW YORK.

ELECTROLYTIC PROCESS OF PRODUCING NITROGEN COM?OUNDS.

To all whom it may concern:

Be it known that I, CHARLES E. ACKER, a citizen of the United States, residing at Niagara Falls, in the county of Niagara and State of New York, have invented certain new and useful Improvements in Electrolytic Processes of Producing Nitrogen Compounds,

of which the following is a specification.

This process relates to the electrolytic production of nitrogen compounds, such as nitrids, amids, cyanamids and cyanids, especially those of the alkali and alkaline-earth metals.

The process comprises the steps of electrolyzing a molten compound of the metal or base which is to be combined with nitrogen, alloying the separated metal with a cathode metal, reacting on the alloyed metal with a nitrogenous gas, and returning the residual metal to the cathode. Incidental steps are the injection of the nitrogenous gas in a direction to cause or assist the circulation of the alloy and residual metal; cooling the althe alloy and residual metal; and successively reacting on the alloyed metal and on the initial roduct of reaction in the presence of the resi ual metal.

Apparatus which may be used in carrying out t e process is shown in the accompanying drawings, in which Figures 1, 2, 3 are vertical longitudinal sections of three diflerent' constructions, each comprising an electrolytic cell and a siparate connected chamber for treating the a 0y; and Fig. 4 illustrates an auxiliary gasabsorbing tower.

Each apparatus illustrated has the general construction of that heretofore devised by me for the production of caustic alkali, the electrolytic cell comprising a cast iron vessel 1 lined at the sides with magnesia brick 2, inclosed in brickwork 3 and covered by a refractory slab 4, through which pass the depending carbon anodes 5. In the bottom of the vessel is a shallow layer 6 of a molten heavy inert metal such as lead, constituting the cathode, upon which is the molten electrolyte 7. The vessel 1.is connected by delivery and return pipes or ducts 8, 9 to a separate chamber 10, into which the nitrogenous as may be introduced by a valved pipe 11. The chamber 10 may be inclosed in the rickwork 3, as shown in Figs. 1, 3, or may be out-v side it as shown in Fig. 2, depending on the Specification of Letters Patent. Application filed October a. 1906. Serial No. 337,976.

Patented March 2, 1909.

.nissun temperature which it is desired to maintain therein.

The delivery pipe 8 of the apparatus shown in Fig. 1 is provided with a series of annular heat-radiating flanges 12, to cool the alloy therein. The delivery pipe 8 of the apparatus shown in Fig. 2 has a lower portion which receives a su plemental gas inlet pipe 13 and thence inc 'nes upward to the chamber 10, the gas injected through the pipe 13 and the initial light compounds produced by the gas rising and moving along the pipe, facilitating the reaction therein. In the apparatus of Fig. 3, a portion of the delivery pipe 8 is enlarged and receives the return pi e 9 so that heat may be transferred from t e outflowing alloy to the returning residual metal. The circulation of the alloy and metal may be eifected either solely by the current of injected gas, as in the apparatus of Figs. 1, 3, or by a mechanical device,

ior 1elxample the screw shown in 2, or by The reaction chamber 10 is of the general construction of that employed in my caustic alkali apparatus, comprising a vertical central pipe 14, which receives the molten alloy and injected gas. The nitrogen compound resulting from the reaction, being usually lighter than the residual metal, rises and collects as a floating la er, which may be run out through a suitab e outlet 15, the metal returning to the electrolytic cell to reconstitute the cathode.

Specific processes which may be carried out are the production ofsodium amid by the injection of ammonia into the molten sodium-lead alloy resulting from the electrolysis of a sodium com ound, such as the chlorid upon a lead cat ode; or the production of calcium nitrid b the injection of nitrogen into an electro ytic calcium-lead alloy. If desired, the alloy may be cooled, wholly or partially, by injecting a regulated amount of a cooled and compressed gaseous reagent, or of a volatile liquid, for example ammonia. The gaseous reagent may be diluted with an inert gas, or mixed with a hydrocarbon gas to produce carbon compounds. Solid carbon or other reagent may be introduced into the reaction chamber/ 10. Alkali-metal cyanide or cyanamlds may be produced in this chamber by first producing sodium amid at a relative y low temperature and then reacting on the amid with carbon or a carbonaceous reagent at a v higher temperature, in the presence of the residual metal. For this purpose it is desirable to first cool the alloy, to prevent decomposition of the injected ammonia by heat, or to employ the expansion of the ammonia to effect this local cooling, and to then retain the heat of reaction and su ply heat by conduction from the electro ytic cell, employing a paratus of the type shown. in Figs. 1 an 3, in which the chamber 10 and cell are inclosed in the same brickwork. In the production of amids, some of the injected ammonia is apt to pass of? without reacting on the sodium in the alloy. This portion of the gas may be recovered by delivering it from the chamber 10 through a pipe '16 into the base of a tower 17, into the top of which water is sprayed through a rose 18. The gas is then recovered from the aqueous solution by distillation and returned to the reaction chamber.

i I claim:

1. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a cathode metal, removing the alloy and reacting on it with a nitrogenous reagent, separating the products of reaction, and returning the residual metal to the cathode.

2. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of ametal capable of forming nitrogen com pounds, alloying the separated metal with a molten cathode metal, removing the molten alloy and reacting on it with a nitrogenous gas, separating the products of reaction, and returning the residual metal to the cathode.

3. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing and cool ing the molten alloy and reacting on it with a nitrogenous gas, separating the products of reactlon, and returning the residual metal to the cathode.

4. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing the 'moltcn alloy and reacting on it with a nitrogenous gas, separating the products of reaction, transferrmg heat from another portion of the molten alloy to the residual metal, and returning the heated metal to the cathode.

5. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound ofa metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing the molten alloy and injecting into it a compressed nitrogenous gas, thereby cooling the alloyand producing a compound, separating the )roducts of reaction, and returning the resi ual metal to the cathode.

6. The electrolytic process of producing nitrogen compounds, which consists in con tinuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing the molten allo and injecting it into a compressed and coo ed nitrogenous gas, thereby cooling the alloy and producing a compound, separating the roducts of reaction, and returning the resir ual metal to the cathode.

7. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing the molten alloy, converting the alloyed metal into a nitrogen compound, and returning the residual metal to the cathode, and producing the nitrogen compound by injecting a nitrogenous gas into the moving alloy.

8. The electrolytic process of producing nitrogen compounds, which consists in continuously electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a molten cathode metal, removing the molten alloy, converting the alloyed metal into a nitrogen compound, and returning the residual metal to the cathode, and producing the nitrogen compound by injecting a nitrogenous gas into tie moving alloy in a'direction to assist the circulation.

9. The electrolytic process of producing alkali-metal amids, which consists in continuously electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with a nitrogenous reagent, separating the resulting amid, and returning the residual metal to the cathode.

10. The electrolytic process of producing alkali-metal amids, which consists in continuously electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkaliand cooling the alloy and reacting on the alloyed metal with ammonia, separating the resulting amid, and returning the residual ietal to the cathode.

12. The electrolytic process of producing alkali-metal amids, which consists in continuously electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with ammonia, separating the resulting amid, returning the residual metal to the cathode, and recovering and utilizing the unabsorbed ammonia.

13. The electrolytic rocess which consists in continuously electro yzing a molten compound with a molten metal cathode, removing and cooling the molten cathode product and reacting on it with a suitable agent, and

returning the residual molten metal to the cathode.

14. The electrolytic rocess which consists in continuously electro yzing a molten compound with a molten metal cathode, removing and cooling the molten cathode product and reacting on it with a suitable agent, returning the residual molten metal to the cathode, and maintaining adjacent but oppositely-directed streams of the cathode product and residual metal to permit the exchange of heat between the streams.

15. A process of making alkali amid, consisting in electrolyzing a molten alkali compound inone vessel in the resence of a molten metal whereby the a kali metal in the compound combines with the molten metal, passing the molton alloy into another vessel in free communication with the former and subjecting said molten alloy to the action of ammonia.

16. A process of making sodium amid, consisting in electrolyzing molten sodium chlorid in one vessel in the presence of a molten metal whereby the sodium combines with the metal, passing the molten alloy into another vessel in free communication with the former and subjecting said molten alloy to the action of ammonia.

17. A process of making sodium amid, consisting in electrolyzing molten sodium chlorid in one vessel in the presence of molten lead whereby the sodium combines with the lead, passing the molten allow into 1 another vessel in free communication with which consists in electrolyzing molten sol dium chlorid in one vessel in the presence of a molten alloying metal, passing the Lmolten sodium alloy into another vessel in i free communication with the first vessel and cooling the alloy, and reacting on the cooled alloy with a nitrogenous reagent.

20. The process of making sodium amid, which. consists in electrolyzing molten sodium chlorid in one vessel in the presence of molten lead, passing the molten sodium-lead alloy into another vessel in free communication with the first vessel and cooling the alloy, and reacting on the cooled alloy with ammonia.

21. The process of producing alkali-metal amids, which consists in electrolyzing a molten alkali-metal com ound in one vessel in the presence of a mo ten alloying metal, passing the molten alloy into another vessel 1n free communication with the first vessel, and reacting on the alloy with a nitrogeneous reagent.

22. The process of producing alkali-metal amids, WhlCh consists in electrolyzing an alkali-metal compound in one vessel in the presence of a suitable liquid metal with which the freed alkali-metal will miX, passing the mixture into another vessel in free communication with the first vessel, and reacting on the mixture with a nitrogeneous reagent.

23. The electrolytic process of producing nitrogen compounds, which consists in electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a cathode metal, removing the alloy and reacting on it with a nitrogenous reagent, separating the products of reaction, and returning the residual metal to the cathode.

24. The electrolytic process of producing alkali-metal amids, which consists in electrolyzing amolten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with a nitrogenous reagent, separating the resulting amid, and returning the residual metal to the cathode.

25. The electrolytic process of producing alkali-metal amids, which consists in electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the alloyed alkali metal with ammonia, separating the resulting amid, and returning the residual metal to the cathode.

26. The electrolytic rocessqof producing nitrogen compounds, w ich consists in electrolyzing a molten compound of a metal capable of forming nitrogen compounds, alloying the separated metal with a cathode metal, removing the molten alloy and reacting on it with a nitrogenous reagent, separating the products of reaction, and returning the residual metal to the cathode.-

27. The electrolytic process of producing alkali-metal amids, which consists in electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the molten alloyed alkali metal with a nitrogenous reagent, separating the resulting amid, and returning the residual metal to the cathode.

28. The electrolytic process of producing 1 alkali-metal amids, which consists in electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal 1 with a cathode metal, removing the alloy and reacting on the molten alloyed alkali metal with ammonia, separating the resultingi amid, and returning the residual metal to the cathode.

29. The electrolytic process of producing nitrogen compounds, which consists in elecl trolyzing a molten compound of a metal ing on it with a nitrogenous reagent, separating the products of reaction, and returning the molten residual metal to the cathode.

30. The electrolytic process of producing alkali-metal amids, which consists in electrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the molten alloyed alkali metal with a nitrogenous reagent, separating the resulting amid, and returning the molten residual metal to the cathode.

81. The electrolytic process of producingalkali-metal amids, which consists inelectrolyzing a molten compound of the alkali metal, alloying the separated alkali metal with a cathode metal, removing the alloy and reacting on the molten alloyed alkali metal with ammonia, separating the result ng amid, I and returning the molten residual metal to the cathode.

In testimony whereof, I alhx my signature in presence of two witnesses.

CHARLES E. ACKER.

/ Witnesses:

OTTO J. JAOOBY, GERALDINE M MCBRIDE. 

